Search results for: Graphite Furnace Atomic Absorption Spectroscopy

Authors: Hamsasew Hankebo Lemago, Dóra Hessz, Tamás Igricz, Zoltán Erdélyi, , Imre Miklós Szilágyi

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Metal oxide inverse opals are a promising class of photocatalysts with a unique hierarchical structure. Atomic layer deposition (ALD) is a versatile technique for the synthesis of high-precision metal oxide thin films, including inverse opals. In this study, we report the synthesis of TiO₂, ZnO, and Al₂O₃ inverse opal and their composites photocatalysts using thermal or plasma-enhanced ALD. The synthesized photocatalysts were characterized using a variety of techniques, including scanning electron microscopy (SEM)-energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), Raman spectroscopy, photoluminescence (PL), ellipsometry, and UV-visible spectroscopy. The results showed that the ALD-synthesized metal oxide inverse opals had a highly ordered structure and a tunable pore size. The PL spectroscopy results showed low recombination rates of photogenerated electron-hole pairs, while the ellipsometry and UV-visible spectroscopy results showed tunable optical properties and band gap energies. The photocatalytic activity of the samples was evaluated by the degradation of methylene blue under visible light irradiation. The results showed that the ALD-synthesized metal oxide inverse opals exhibited high photocatalytic activity, even under visible light irradiation. The composites photocatalysts showed even higher activity than the individual metal oxide inverse opals. The enhanced photocatalytic activity of the composites can be attributed to the synergistic effect between the different metal oxides. For example, Al₂O₃ can act as a charge carrier scavenger, which can reduce the recombination of photogenerated electron-hole pairs. The ALD-synthesized metal oxide inverse opals and their composites are promising photocatalysts for a variety of applications, such as wastewater treatment, air purification, and energy production. The ALD-synthesized metal oxide inverse opals and their composites are promising photocatalysts for a variety of applications, such as wastewater treatment, air purification, and energy production.

Keywords: ALD, metal oxide inverse opals, photocatalysis, composites

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Authors: Ling Dai

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Surface-sensing devices such as atomic force microscope have been widely used to characterize the surface structure and properties of nanoscale polymer films. However, using molecular dynamics simulations, we show that there is intrinsic and unavoidable inelastic deformation at polymer surfaces induced by the sensing tip. For linear chain polymers like perfluoropolyether, such tip-induced deformation derives from the differences in the atomic interactions which are atomic specie-based Van der Waals interactions, and resulting in atomic shuffling and causing inelastic alternation in both molecular structures and mechanical properties at the regions of the polymer surface. For those aromatic chain polymers like epoxy, the intrinsic deformation is depicted as the intra-chain rotation of aromatic rings and kinking of linear atomic connections. The present work highlights the need to reinterpret the data obtained from surface-sensing tests by considering this intrinsic inelastic deformation occurring at polymer surfaces.

Keywords: polymer, surface, nano, molecular dynamics

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Authors: S. Zhuiykov, E. Kats

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Electrical properties and morphology of orthorhombic β–WO3 nano-flakes with thickness of ~7-9 nm were investigated at the nano scale using energy dispersive X-ray diffraction (XRD), X-ray photo electron spectroscopy (XPS) and current sensing force spectroscopy atomic force microscopy (CSFS-AFM, or PeakForce TUNATM). CSFS-AFM analysis established good correlation between the topography of the developed nano-structures and various features of WO3 nano-flakes synthesized via a two-step sol-gel-exfoliation method. It was determined that β–WO3 nano-flakes annealed at 550ºC possess distinguished and exceptional thickness-dependent properties in comparison with the bulk, micro- and nano-structured WO3 synthesized at alternative temperatures.

Keywords: electrical properties, layered semiconductors, nano-flake, sol-gel, exfoliation WO3

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Authors: Aubrey Langeland, Richard Neitzel, Kowit Nambunmee

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Electronic waste, ‘e-waste’, refers generally to discarded electronics and electrical equipment, including products from cell phones and laptops to wires, batteries and appliances. While e-waste represents a transformative source of income in low- and middle-income countries, informal e-waste workers use rudimentary methods to recover materials, simultaneously releasing harmful chemicals into the environment and creating a health hazard for themselves and surrounding communities. Valuable materials such as precious metals, copper, aluminum, ferrous metals, plastic and components are recycled from e-waste. However, persistent organic pollutants such as polychlorinated biphenyls (PCBs) and some polybrominated diphenyl ethers (PBDEs), and heavy metals are toxicants contained within e-waste and are of great concern to human and environmental health. The current study seeks to evaluate the environmental contamination resulting from informal e-waste recycling in a predominantly agricultural community in northeastern Thailand. To accomplish this objective, five types of environmental samples were collected and analyzed for concentrations of eight metals commonly associated with e-waste recycling during the period of July 2016 through July 2017. Rice samples from the community were collected after harvest and analyzed using inductively coupled plasma mass spectrometry (ICP-MS) and gas furnace atomic spectroscopy (GF-AS). Soil samples were collected and analyzed using methods similar to those used in analyzing the rice samples. Surface water samples were collected and analyzed using absorption colorimetry for three heavy metals. Environmental air samples were collected using a sampling pump and matched-weight PVC filters, then analyzed using Inductively Coupled Argon Plasma-Atomic Emission Spectroscopy (ICAP-AES). Finally, surface wipe samples were collected from surfaces in homes where e-waste recycling activities occur and were analyzed using ICAP-AES. Preliminary1 results indicate that some rice samples have concentrations of lead and cadmium significantly higher than limits set by the United States Department of Agriculture (USDA) and the World Health Organization (WHO). Similarly, some soil samples show levels of copper, lead and cadmium more than twice the maximum permissible level set by the USDA and WHO, and significantly higher than other areas of Thailand. Surface water samples indicate that areas near e-waste recycling activities, particularly the burning of e-waste products, result in increased levels of cadmium, lead and copper in surface waters. This is of particular concern given that many of the surface waters tested are used in irrigation of crops. Surface wipe samples measured concentrations of metals commonly associated with e-waste, suggesting a danger of ingestion of metals during cooking and other activities. Of particular concern is the relevance of surface contamination of metals to child health. Finally, air sampling showed that the burning of e-waste presents a serious health hazard to workers and the environment through inhalation and deposition2. Our research suggests a need for improved methods of e-waste recycling that allows workers to continue this valuable revenue stream in a sustainable fashion that protects both human and environmental health. 1Statistical analysis to be finished in October 2017 due to follow-up field studies occurring in July and August 2017. 2Still awaiting complete analytic results.

Keywords: e-waste, environmental contamination, informal recycling, metals

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Authors: R. S. Yadav, J. Havlica, I. Kuřitka, Z. Kozakova, J. Masilko, L. Kalina, M. Hajdúchová, V. Enev, J. Wasserbauer

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Nickel spinel ferrite NiFe2O4 nanoparticles with different particle size at different annealing temperature were synthesized using the starch-assisted sol-gel auto-combustion method. The synthesized nanoparticles were characterized by conventional powder X-ray diffraction (XRD) spectroscopy, Raman Spectroscopy, Fourier Transform Infrared Spectroscopy, Field-Emission Scanning Electron Microscopy, X-ray Photoelectron Spectroscopy and Vibrating Sample Magnetometer. The XRD patterns confirmed the formation of NiFe2O4 spinel ferrite nanoparticles. Field-Emission Scanning Electron Microscopy revealed that particles are of spherical morphology with particle size 5-20 nm at lower annealing temperature. An infrared spectroscopy study showed the presence of two principal absorption bands in the frequency range around 525 cm-1 (ν1) and around 340 cm-1 (ν2); which indicate the presence of tetrahedral and octahedral group complexes, respectively, within the spinel ferrite nanoparticles. Raman spectroscopy study also indicated the change in octahedral and tetrahedral site related Raman modes in nickel ferrite nanoparticles with change of particle size. This change in magnetic behavior with change of particle size of NiFe2O4 nanoparticles was observed.

Keywords: nickel ferrite, nanoparticles, magnetic property, NiFe2O4

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Authors: Jose Alberto Duarte Moller, Cynthia Deisy Gomez Esparza

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The cobalt-titanium system was grown as thin films in an INTERCOVAMEX V3 sputtering system, equipped with four magnetrons assisted by DC pulsed and direct DC. A polished highly oriented (400) silicon wafer was used as substrate and the growing temperature was 500 oC. Xray Absorption Spectroscopy experiments were carried out in the SSRL in the 4-3 beam line. The Extenden X-Ray Absorption Fine Structure spectra have been numerically processed by WINXAS software from the background subtraction until the normalization and FFT adjustment. Analyzing the absorption spectra of cobalt in the CoTi2 phase we can appreciate that they agree in energy with the reference spectra that corresponds to the CoO, which indicates that the valence where upon working is Co2+. The RDF experimental results were then compared with those RDF´s generated theoretically by using FEFF software, from a model compound of CoTi2 phase obtained by XRD. The fitting procedure is a highly iterative process. Fits are also checked in R-space using both the real and imaginary parts of Fourier transform. Finally, the presence of overlapping coordination shells and the correctness of the assumption about the nature of the coordinating atom were checked.

Keywords: XAS, EXAFS, FEFF, CoTi

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Authors: Nor Sayzwani Sukri, Siti Hajar Ya’acob, Musfiroh Jani, Farah Khaliz Kedri, Noor Syuhadah Subki, Zulhazman Hamzah

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In mid-December 2014, the biggest flood event occurred in East Coast of Peninsular Malaysia especially at Dabong area, Kelantan. As a consequent of flood disaster, the heavy metals concentration in soil may changes and become harmful to the environment due to the pollution that deposited in soil. This study was carried out to determine the heavy metal concentration from flood affected area. Sample have been collected and analysed by using Atomic Absorption Spectroscopy (AAS). Lead (Pb), Cadmium (Cd), Mercury (Hg), and Arsenic (As) were chosen for the heavy metals concentration. The result indicated that the heavy metal concentration did not exceed the limit. In-situ parameters also were carried out, were the results showed the range of soil pH (6.5-6.8), temperature (25°C – 26.5°C), and moisture content (1-2), respectively. The results from this study can be used as a base data to improve the soil quality and for consideration of future land use activities.

Keywords: flood, soil, heavy metal, AAS

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Authors: Raphael Odoh, Obida J. Oko, Mary S. Dauda

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The determination of Cd, Cr, Cu, Fe,Mn, Ni, Pb and Zn contents in edible oils (palm oil, ground-nut oil and soybean oil) bought from various markets of Benue and Taraba state were carried out with flame atomic absorption spectrophotometric technique. The method 3031 developed acid digestion of oils for metal analysis by atomic absorption or ICP spectrometry was used in the preparation of the edible oil samples for the determination of total metal content in this study. The overall results (µg/g) in palm oil sample ranged from 0.028-0.076, 0.035-0.092, 1.011-1.955, 2.101-4.892, 0.666-0.922, 0.054-0.095, 0.031-0.068 and 1.987-2.971 for Cd, Cr, Cu, Fe, Mn, Ni, Pb and Zn respectively, while in ground-nut oil the overall results ranged from 0.011-0.042, 0.011-0.052, 0.133-0.788, 1.789-2.511, 0.078-0.765, 0.045-0.092, 0.011-0.028 and 1.098-1.997 for Cd, Cr, Cu, Fe, Mn, Ni, Pb and Zn respectively. Of the heavy metals considered Cd and Ni showed the highest contamination in the soybean oil sample. The overall results in soybean oil samples ranged from 0.011-0.015, 0.017-0.032, 0.453-0.987, 1.789-2.511, 0.089-0.321, 0.011-0.016, 0.012-0.065 and 1.011-1.997 for Cd, Cr, Cu, Fe, Mn, Ni, Pb and Zn respectively. The concentration of Pb was the highest. The degree of contamination by each metal was estimated by the transfer factor. The transfer factors obtained for Cd, Cr, Cu, Fe, Mn, Ni, Pb and Zn in edible oils (palm oil, ground-nut oil and soybean oil) were 10.800, 16.500, 16.000, 18.813, 15.115, 14.230, 23.000 and 9.418 for Cd, Cr, Cu, Fe, Mn, Ni, Pb and Zn in palm oil, and 7.000, 12.500, 8.880, 11.333, 7.708, 10.833, 15.00 and 6.608 for Cd, Cr, Cu, Fe, Mn, Ni, Pb and Zn in ground-nut oil while for soybean oil the transfer factors were 13.000, 11.000, 7.642, 11.578, 4.486, 13.00, 12.333 and 4.412 for Cd, Cr, Cu, Fe, Mn, Ni, Pb and Zn respectively. The inter-element correlation was found among metals in edible oil samples using Pearson’s correlation co-efficient. There were positive and negative correlations among the metals determined. All Metals determined showed degree of contamination but concentrations lower than the USP specification.

Keywords: Benue State, contamination, edible oils, heavy metals, markets, Taraba State

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Authors: Majid Samavatian, Reza Gholamipour, Vahid Samavatian

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This study addresses the role of rejuvenation on the fluctuation of atomic-level stresses and nanoscale topological heterogeneity in ZrCuNiAl bulk metallic glass (BMG). Based on atomic force microscopy (AFM) results, the rejuvenation process leads to an increase in nanoscale spatial heterogeneity manifested by the intensification of the local viscoelastic response of the BMG nanostructure. It means that the rejuvenation process induces more loose-packing structures which behave towards an external load in a viscoelastic way. Hence, it is suggested that the alteration of such heterogeneity may be attributed to the variation of positional atomic rearrangement during the evolution of structural rejuvenation. On the other side, the synchrotron X-ray diffraction (XRD) results indicate that the rejuvenation intensifies the variation of internal stresses at the atomic level. This conclusion unfolds that the increase of atomic-level stresses during rejuvenation induces structural disordering and nanoscale heterogeneity in the amorphous material.

Keywords: bulk metallic glass, heterogeneity, rejuvenation, nanostructure

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Authors: S. Krustev, V. Angelova, K. Ivanov, P. Zaprjanova

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Approximately a dozen trace elements are vital for the development of all plants and some other elements are significant for some species. Heavy metals do not belong to this group of elements that are essential to plants, but some of them such as copper and zinc, have a dual effect on their growth. Concentration levels of these elements in the different regions of the world vary considerably. Their high concentrations in some parts of Central and Eastern Europe cause concern for human health and degrade the quality of agricultural produce from these areas. This study aims to compare the prevalence and levels of the major trace elements in some rural areas of Central and Eastern Europe. Soil samples from different regions of the Czech Republic, Slovakia, Austria, Hungary, Serbia, Romania, Bulgaria and Greece far from large industrial centers have been studied. The main methods for their determination are the atomic spectral techniques – atomic absorption and plasma atomic emission. As a result of this study, data on microelements levels in soils of 17 points from the main grain-producing regions of Central and Eastern Europe are presented and systematized. The content of trace elements was in the range of 5.0-84.1 mg.kg⁻¹ for Cu, 0.3-1.4 mg.kg⁻¹ for Cd, 26.1-225.5 mg.kg⁻¹ for Zn, 235.5-788.6 mg.kg⁻¹ for Mn and 4.1-25.8 mg.kg⁻¹ for Pb.

Keywords: trace elements, heavy metals, agricultural soils, Central and Eastern Europe

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Authors: Jian Zheng

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Three-dimensional (3D) network structure has been recognized as an effective approach to enhance the mechanical and thermal conductive properties of polymeric composites. However, it has not been applied in energetic materials. In this work, a fluoropolymer based composite with vertically oriented and interconnected 3D graphite network was fabricated for polymer bonded explosives (PBXs). Here, the graphite and graphene oxide platelets were mixed, and self-assembled via rapid freezing and using crystallized ice as the template. The 3D structure was finally obtained by freezing-dry and infiltrating with the polymer. With the increasing of filler fraction and cooling rate, the thermal conductivity of the polymer composite was significantly improved to 2.15 W m⁻¹ K⁻¹ by 1094% than that of pure polymer. Moreover, the mechanical properties, such as tensile strength and elastic modulus, were enhanced by 82% and 310%, respectively, when the highly ordered structure was embedded in the polymer. We attribute the increased thermal and mechanical properties to this 3D network, which is beneficial to the effective heat conduction and force transfer. This study supports a desirable way to fabricate the strong and thermal conductive fluoropolymer composites used for the high-performance polymer bonded explosives (PBXs).

Keywords: mechanical properties, oriented network, graphite polymer composite, thermal conductivity

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Authors: C. L. Popa, S. L. Iconaru, A. Costescu, C. S. Ciobanu, M. Motelica Heino, R. Guegan, D. Predoi

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Surface functionalization of ceramic composites with a special focus on tetraethyl orthosilicate (TEOS) and hydroxyapatite (HAp) is discoursed. Mesoporous ceramic HAp-TEOS composites were prepared by the incorporation of hydroxyapatite into tetraethyl orthosilicate by sol-gel method. The resulting samples were analysed by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared (FT-IR) spectroscopy, and Raman spectroscopy and nitrogen physisorption. The removal of Pb2+ ions from aqueous solutions was evaluated using Atomic Absorbtion Spectroscopy (AAS). Removal experiments of Pb2+ ions were carried out in aqueous solutions with controlled Pb2+ at pH ~ 3 and pH ~ 5. After removal experiment of Pb2+ at pH 3 and pH 5, porous hydroxyapatite nanoparticles is transformed into PbHAp_3 and PbHAp_5 via the adsorption of Pb2+ ions followed by the cation exchange reaction. The diffraction patterns show that THAp nanoparticles were successfully coated with teos without any structural changes. On the other, the AAS analysis showed that THAp can be useful in the removal Pb2+ from water contaminated.

Keywords: teos, hydroxyapatite, environment applications, biosystems engineering

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Authors: Shivalinge Gowda

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The total mass attenuation coefficients m/r, of some halides such as, NaCl, KCl, CuCl, NaBr, KBr, RbCl, AgCl, NaI, KI, AgBr, CsI, HgCl₂, CdI₂ and HgI₂ were determined at photon energies 279.2, 320.07, 514.0, 661.6, 1115.5, 1173.2 and 1332.5 keV in a well-collimated narrow beam good geometry set-up using a high resolution, hyper pure germanium detector. The mass attenuation coefficients and the effective atomic cross sections are found to be in good agreement with the XCOM values. From these mass attenuation coefficients, the effective atomic cross sections s_a, of the compounds were determined. These effective atomic cross section s_a data so obtained are then used to compute the effective atomic numbers Z_eff. For this, the interpolation of total attenuation cross-sections of photons of energy E in elements of atomic number Z was performed by using the logarithmic regression analysis of the data measured by the authors and reported earlier for the above said energies along with XCOM data for standard energies. The best-fit coefficients in the photon energy range of 250 to 350 keV, 350 to 500 keV, 500 to 700 keV, 700 to 1000 keV and 1000 to 1500 keV by a piecewise interpolation method were then used to find the Z_eff of the compounds with respect to the effective atomic cross section s_a from the relation obtained by piece wise interpolation method. Using these Z_eff values, the electron densities N_el of halides were also determined. The present Z_eff and N_el values of halides are found to be in good agreement with the values calculated from XCOM data and other available published values.

Keywords: mass attenuation coefficient, atomic cross-section, effective atomic number, electron density

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Authors: Bireswar Paul, Amitava Datta

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Indoor air environment is a big concern in the last few decades in the developing countries, with increased focus on monitoring the air quality. In this work, an experimental study has been conducted to establish the existence of carbon nanoparticles below the size range of 10 nm in the non-sooting zone of a LPG/air partially premixed flame. Mainly, four optical techniques, UV absorption spectroscopy, fluorescence spectroscopy, dynamic light scattering and TEM have been used to characterize and measure the size of carbon nanoparticles in the sampled materials collected from the inner surface of the flame front. The existence of the carbon nanoparticles in the sampled material has been confirmed with the typical nature of the absorption and fluorescence spectra already reported in the literature. The band gap energy shows that the particles are made up of three to six aromatic rings. The size measurement by DLS technique also shows that the particles below the size range of 10 nm. The results of DLS are also corroborated by the TEM image of the same material. 

Keywords: indoor air, carbon nanoparticle, lpg, partially premixed flame, optical techniques

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Authors: M. Muneer, Waseem Raza

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Nano-crystalline materials of pure and metal-doped semiconducting materials have been successfully synthesized using sol gel and hydrothermal methods. The prepared materials were characterized by standard analytical techniques, i.e., XRD, SEM, EDX, UV–vis Spectroscopy and FTIR. The (XRD) analysis showed that the obtained particles are present in partial crystalline nature and exhibit no other impurity phase. The EDX and (SEM) images depicted that metals have been successfully loaded on the surface of the semiconductor. FTIR showed an additional absorption band at 910 cm−1, characteristic of absorption band indicating the incorporation of dopant into the lattice in addition to a broad and strong absorption band in the region of 410–580 cm−1 due to metal–O stretching. The UV–vis absorption spectra of synthesized particles indicate that the doping of metals into the lattice shift the absorption band towards the visible region. Thermal analysis, measurement of the synthesized sample showed that the thermal stability of pure semiconducting material is decreased due to increase in dopant concentration. The photocatalytic activity of the synthesized particles was studied by measuring the change in concentration of three different chromophoric dyes as a function of irradiation time. The photocatalytic activity of doped materials were found to increase with increase in dopant concentration.

Keywords: photocatalysis, metal doped semicondcutors, dye degradation, visible light active materials

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Authors: Soner Cubuk, Mirgul Kosif, M. Vezir Kahraman, Ece Kok Yetimoglu

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Boron is an essential trace element for the completion of the life circle for organisms. Suitable methods for the determination of boron have been proposed, including acid - base titrimetric, inductively coupled plasma emission spectroscopy flame atomic absorption and spectrophotometric. However, the above methods have some disadvantages such as long analysis times, requirement of corrosive media such as concentrated sulphuric acid and multi-step sample preparation requirements and time-consuming procedures. In this study, a selective and reusable fluorescent sensor for boron based on glycosyloxyethyl methacrylate was prepared by photopolymerization. The response characteristics such as response time, pH, linear range, limit of detection were systematically investigated. The excitation/emission maxima of the membrane were at 378/423 nm, respectively. The approximate response time was measured as 50 sec. In addition, sensor had a very low limit of detection which was 0.3 ppb. The sensor was successfully used for the determination of boron in water samples with satisfactory results.

Keywords: boron, fluorescence, photopolymerization, polymeric sensor

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Authors: Shahrazed Medeghri, Saad Hamzaoui, Mokhtar Zerdali

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The metallurgical grade silicon (MG-Si) is obtained from the reduction of silica (SiO₂) in an induction furnace or an electric arc furnace. Impurities inherent in reduction process also depend on the quality of the raw material used. Among the applications of the silicon, it is used as a substrate for the photovoltaic conversion of solar energy and this conversion is wider as the purity of the substrate is important. Research is being done where the purpose is looking for new methods of manufacturing and purification of silicon, as well as new materials that can be used as substrates for the photovoltaic conversion of light energy. In this research, the technique of production of silicon in an induction furnace, using a high vacuum for fusion. Diatomaceous Silica (SiO2) used is 99 mass% initial purities, the carbon used is 6N of purity and the particle size of 63μm as starting materials. The final achieved purity of the material was above 50% by mass. These results demonstrate that this method is a technically reliable, and allows obtaining a better return on the amount 50% of silicon.

Keywords: induction furnaces, amorphous silica, carbon microstructure, silicon

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Authors: Philipp Stehle, Dragoljub Vrankovic, Montaha Anjass

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Due to its high availability and extremely high specific capacity, silicon (Si) is the most promising anode material for next generation lithium-ion batteries (LIBs). However, Si anodes are suffering from high volume changes during cycling causing unstable solid-electrolyte interface (SEI). One approach for mitigation of these effects is to embed Si particles into a carbon matrix to create silicon/carbon composites (Si/C). These typically show more stable electrochemical performance than bare silicon materials. Nevertheless, the same failure mechanisms mentioned earlier appear in a less pronounced form. In this work, we further improved the cycling performance of two commercially available Si/C materials by coating thin metal oxide films of different thicknesses on the powders via Atomic Layer Deposition (ALD). The coated powders were analyzed via ICP-OES and AFM measurements. Si/C-graphite anodes with automotive-relevant loadings (~3.5 mAh/cm2) were processed out of the materials and tested in half coin cells (HCCs) and full pouch cells (FPCs). During long-term cycling in FPCs, a significant improvement was observed for some of the ALD-coated materials. After 500 cycles, the capacity retention was already up to 10% higher compared to the pristine materials. Cycling of the FPCs continued until they reached a state of health (SOH) of 80%. By this point, up to the triple number of cycles were achieved by ALD-coated compared to pristine anodes. Post-mortem analysis via various methods was carried out to evaluate the differences in SEI formation and thicknesses.

Keywords: silicon anodes, li-ion batteries, atomic layer deposition, silicon-carbon composites, surface coatings

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Authors: Swapna Koneru, Srinivasa Rao Allam, Vijaya Prakash Gaddem

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The different concentrations of neodymium-doped (Nd-doped) oxy fluoroborate (OFB) glasses were prepared by melt quenching method and characterized through optical absorption, emission and decay curve measurements to understand the lasing potentialities of these glasses. Optical absorption spectra were recorded and have been analyzed using Judd–Ofelt theory. The dipole strengths are parameterized in terms of three phenomenological Judd–Ofelt intensity parameters Ωλ (λ=2, 4 and 6) to elucidate the glassy matrix around Nd3+ ion as well as to determine the 4F3/2 metastable state radiative properties such as the transition probability (AR), radiative lifetime (τR), branching ratios (βR) and integrated absorption cross-section (σa) have been measured for most of the fluorescent levels of Nd3+. The emission spectra recorded for these glasses exhibit two peaks at 1085 and 1328 nm corresponding to 4F3/2 to 4I11/2 and 4I13/2 transitions have been obtained for all the glasses upon 808 nm diode laser excitation in the near infrared region. The emission intensity of the 4F3/2 to 4I11/2 transition increases with increase of Nd3+ concentration up to 1 mol% and then concentration quenching is observed for 2.0 mol% of Nd3+ concentration. The lifetimes for the 4F3/2 level are found to decrease with increase in Nd2O3 concentration in the glasses due to the concentration quenching. The decay curves of all these glasses show single exponential behavior. The spectroscopy of Nd3+ in these glasses is well understood and laser properties can be accurately determined from measured spectroscopic properties. The results obtained are compared with reports on similar glasses. The results indicate that the present glasses could be useful for 1.08 µm laser applications.

Keywords: glasses, luminescence, optical properties, photoluminescence spectroscopy

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Authors: Julien Acquadro, Sophie Noel, Frédéric Houze, Philippe Teste, Pascal Chretien, Clément Genet, Edouard Breniaux, Marie-Joël Menu, Florence Ansart, Marie Gressier

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This paper presents the study results of the electrical and tribological properties of nanocomposite hybrid sol-gel coatings developed for industrial applications on electrical connector housings. The electrical properties of coatings are provided by conductive fillers. The coatings presented in this study are formulated with different types of conductive carbon fillers, in this case carbon black and graphite particles. The coatings are deposited on a high-phosphorous nickel substrate by a dip-coating process. The authors have investigated the effects of the carbon black/graphite ratio on the coating's electrical and tribological properties. Electrical characterizations with a 4-probe method and AFM measurements as well as tribological tests by micro-friction shed light on the role of the black carbon/graphite ratio on the final properties of the sol-gel nanocomposite coatings. This study shows that the amount of carbon black mainly drives the coatings' electrical conduction property, while graphite's lubrication properties bring interest to reduce the values of friction coefficients (at a contact pressure of 800 MPa). In the industrial field of electrical connectors, such coatings aim at replacing cadmium and chromium (VI) protection, as recommended by REACH (Registration, Evaluation and Authorization of Chemicals) and RoHS (Restriction of Hazardous Substances in electrical and electronic equipment) regulations (Annex XVII of REACH).

Keywords: carbon conductive fillers, electrical conduction, sol-gel coatings, tribology

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Authors: Chi-Yan Chu, Kai-Chi Chuang, Huang-Chung Cheng

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In this study, the RRAM devices with the TiN/Ti/HfO_x/TiN structure were fabricated, then the electrical characteristics of the devices without annealing and after 400 °C and 500 °C of the furnace annealing (FA) temperature processes were compared. The RRAM devices after the FA’s 400 °C showed the lower forming, set and reset voltages than the other devices without annealing. However, the RRAM devices after the FA’s 500 °C did not show any electrical characteristics because the TiN/Ti/HfO_x/TiN device was oxidized, as shown in the XPS analysis. From these results, the RRAM devices after the FA’s 400 °C showed the best electrical characteristics.

Keywords: RRAM, furnace annealing (FA), forming, set and reset voltages, XPS

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Authors: Hossein Navid, Maryam Adeli Khadem, Shahin Oustan, Mahmoud Zareie

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Among the nutrients needed by the plants, three elements containing nitrate, phosphorus and potassium are more important. The objective of this research was measuring these nutrient amounts in soil using Fourier transform infrared spectroscopy in range of 400- 4000 cm-1. Soil samples for different soil types (sandy, clay and loam) were collected from different areas of East Azerbaijan. Three types of fertilizers in conventional farming (urea, triple superphosphate, potassium sulphate) were used for soil treatment. Each specimen was divided into two categories: The first group was used in the laboratory (direct measurement) to extract nitrate, phosphorus and potassium uptake by colorimetric method of Olsen and ammonium acetate. The second group was used to measure drug absorption spectrometry. In spectrometry, the small amount of soil samples mixed with KBr and was taken in a small pill form. For the tests, the pills were put in the center of infrared spectrometer and graphs were obtained. Analysis of data was done using MINITAB and PLSR software. The data obtained from spectrometry method were compared with amount of soil nutrients obtained from direct drug absorption using EXCEL software. There were good fitting between these two data series. For nitrate, phosphorus and potassium R2 was 79.5%, 92.0% and 81.9%, respectively. Also, results showed that the range of MIR (mid-infrared) is appropriate for determine the amount of soil nitrate and potassium and can be used in future research to obtain detailed maps of land in agricultural use.

Keywords: nitrate, phosphorus, potassium, soil nutrients, spectroscopy

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Authors: Wan-Tzu Yen, Yu-Chen Luo, I-Ping Liu, Po-Hsuan Yeh, Sheng-Hsun Fu, Yuh-Lang Lee

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Self-assembled characteristics and adsorption performance of 1-dodecylamine molecules on gold (Au) (111) surfaces were characterized via cyclic voltammetry (CV), surface-enhanced infrared absorption spectroscopy (SEIRAS) and scanning tunneling microscopy (STM). The present study focused on the formation of 1-dodecylamine (DDA) on a gold surface with respect to the ex-situ arrangement of an adlayer on the Au(111) surface, and phase transition at potential dynamics carried out by EC-STM. This study reveals that alkyl amine molecules were formed an adsorption pattern with highly regular “lie down shape” on Au(111) surface, even in an extreme acid system (pH = 1). Acidic electrolyte (HClO₄) could protonate the surface of alkyl amine of a monolayer of the gold surface when potential shifts to negative. The quite stability of 1-dodecylamine on the gold surface maintained the monolayer across the potential window (0.1-0.8V). This transform model was confirmed by EC-STM. In addition, amine-modified Au(111) electrode adlayer used to examine how to affect an electron transfer across an interface using [Fe(CN)₆]³⁻/[Fe(CN)₆]⁴⁻ redox pair containing 0.1 M HClO₄ solution.

Keywords: cyclic voltammetry, dodecylamine, gold (Au)(111), scanning tunneling microscopy, self-assembled monolayer, surface-enhanced infrared absorption spectroscopy

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Authors: Elena Ionescu, Elena Iacob, Marie-Louise Ionescu, Carmen Elena Tebrencu, Oana Teodora Ciuperca

Abstract:

Echinacea species (Asteraceae) has received a global attention because it is widely used for treatment of cold, flu and upper respiratory tract infections. Echinacea species contain a great variety of chemical components that contribute to their activity. The most important components responsible for the biological activity are those with high molecular-weight such as polysaccharides, polyacetylenes, highly unsaturated alkamides and caffeic acid derivatives. The principal factors that may influence the chemical composition of Echinacea include the species and the part of plant used (aerial parts or roots ). In recent years the market for Echinacea has grown rapidly and also the cases of adultery/replacement especially for Echinacea root. The identification of presence or absence of same biomarkers provide information for safe use of Echinacea species in food supplements industry. The aim of the study was the preliminary evaluation and fingerprinting by UV-VISIBLE spectroscopy of biomarkers in terms of content in phenolic derivatives of some Echinacea species (E. purpurea, E. angustifolia and E. pallida) for identification and authentication of the species. The steps of the study were: (1) samples (extracts) preparation from Echinacea species (non-hydrolyzed and hydrolyzed ethanol extracts); (2) samples preparation of reference substances (polyphenol acids: caftaric acid, caffeic acid, chlorogenic acid, ferulic acid; flavonoids: rutoside, hyperoside, isoquercitrin and their aglycones: quercitri, quercetol, luteolin, kaempferol and apigenin); (3) identification of specific absorption at wavelengths between 700-200 nm; (4) identify the phenolic compounds from Echinacea species based on spectral characteristics and the specific absorption; each class of compounds corresponds to a maximum absorption in the UV spectrum. The phytochemical compounds were identified at specific wavelengths between 700-200 nm. The absorption intensities were measured. The obtained results proved that ethanolic extract showed absorption peaks attributed to: phenolic compounds (free phenolic acids and phenolic acids derivatives) registrated between 220-280 nm, unsymmetrical chemical structure compounds (caffeic acid, chlorogenic acid, ferulic acid) with maximum absorption peak and absorption "shoulder" that may be due to substitution of hydroxyl or methoxy group, flavonoid compounds (in free form or glycosides) between 330-360 nm, due to the double bond in position 2,3 and carbonyl group in position 4 flavonols. UV spectra showed two major peaks of absorption (quercetin glycoside, rutin, etc.). The results obtained by UV-VIS spectroscopy has revealed the presence of phenolic derivatives such as cicoric acid (240 nm), caftaric acid (329 nm), caffeic acid (240 nm), rutoside (205 nm), quercetin (255 nm), luteolin (235 nm) in all three species of Echinacea. The echinacoside is absent. This profile mentioned above and the absence of phenolic compound echinacoside leads to the conclusion that species harvested as Echinacea angustifolia and Echinacea pallida are Echinacea purpurea also; It can be said that preliminary fingerprinting of Echinacea species through correspondence with the phenolic derivatives profile can be achieved by UV-VIS spectroscopic investigation, which is an adequate technique for preliminary identification and authentication of Echinacea in medicinal herbs.

Keywords: Echinacea species, Fingerprinting, Phenolic compounds, UV-VIS spectroscopy

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Authors: Edgar Aguilar-Ortíz, Nicolas Lévaray, Mireille Vonlanthen, Eric G. Morales-Espinoza, Ernesto Rivera, Xiao Xia Zhu

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Four new star compounds bearing a porphyrin core and cholic acid units, (TPPh(Zn) tetra-CA, TPPh(2H) tetra-CA, TPPh(Zn) octa-CA and TPPh(2H) octa-CA), have been synthesized using the Click Chemistry approach, which consist on azide-alkyne couplings. These novel functionalized porphyrins were characterized by 1H and 13C NMR spectroscopy and their structure was confirmed by MALDI-TOF. The optical properties of these compounds were studied by absorption and fluorescence spectroscopy. On the other hand, order to evaluate the amphiphilic properties of the cholic acid units combined with the optical response of the porphyrin core, we performed absorption and fluorescence studies in function of the polarity of the environment. It was found that as soon as we increase the polarity of the solvent, the Zn-metallated porphyrins, (TPPh(Zn) tetra-CA and TPPh(Zn) octa-CA), are able to form J aggregates, whereas the free-base porphyrins, TPPh(2H) tetra-CA and TPPh(2H) octa-CA, behaved differently.

Keywords: aggregates, amphiphilic, cholic acid, click-chemistry, porphyrin

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Authors: Ali N. Siyal, Saima Q. Memon, Latif Elçi, Aydan Elçi

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Polystyrene (PS) was extracted from Styrofoam (expanded polystyrene foam) waste, so called white pollutant. The PS was functionalized with N, N- Bis(2-aminobenzylidene)benzene-1,2-diamine (ABA) ligand through an azo spacer. The resin was characterized by FT-IR spectroscopy and elemental analysis. The PS-N=N-ABA resin was used for the enrichment and speciation of Cr(III)/Cr(VI) ions and total Cr determination in aqueous samples by Flame Atomic Absorption Spectrometry (FAAS). The separation of Cr(III)/Cr(VI) ions was achieved at pH 2. The recovery of Cr(VI) ions was achieved ≥ 95.0% at optimum parameters: pH 2; resin amount 300 mg; flow rates 2.0 mL min-1 of solution and 2.0 mL min-1 of eluent (2.0 mol L-1 HNO3). Total Cr was determined by oxidation of Cr(III) to Cr(VI) ions using H2O2. The limit of detection (LOD) and quantification (LOQ) of Cr(VI) were found to be 0.40 and 1.20 μg L-1, respectively with preconcentration factor of 250. Total saturation and breakthrough capacitates of the resin for Cr(IV) ions were found to be 0.181 and 0.531 mmol g-1, respectively. The proposed method was successfully applied for the preconcentration/speciation of Cr(III)/Cr(VI) ions and determination of total Cr in industrial effluents.

Keywords: styrofoam waste, polymeric resin, preconcentration, speciation, Cr(III)/Cr(VI) ions, FAAS

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Authors: Yang Song, Xiaojun Qiu

Abstract:

Multilayer materials are applied to much acoustics area. Multilayer porous materials are dominant in room absorber. Multilayer viscoelastic materials are the basic parts in underwater absorption coating. In most cases, the one-way sound absorption performance of multilayer material is concentrated according to the sound source site. But the two-way sound absorption performance is also necessary to be known in some special cases which sound is produced in both sides of the material and the both sides especially might contact with different media. In this article, this kind of case was research. The multilayer material was composed of viscoelastic layer and steel plate and the porous layer. The two sides of multilayer material contact with water and air, respectively. A theory model was given to describe the sound propagation and impedance in multilayer absorption material. The two-way sound absorption properties of several multilayer materials were calculated whose two sides all contacted with different media. The calculated results showed that the difference of two-way sound absorption coefficients is obvious. The frequency, the relation of layers thickness and parameters of multilayer materials all have an influence on the two-way sound absorption coefficients. But the degrees of influence are varied. All these simulation results were analyzed in the article. It was obtained that two-way sound absorption at different frequencies can be promoted by optimizing the configuration parameters. This work will improve the performance of underwater sound absorption coating which can absorb incident sound from the water and reduce the noise radiation from inside space.

Keywords: different media, multilayer material, sound absorption coating, two-way sound absorption

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Authors: Shigeyuki Haruyama, Oke Oktavianty, Zefry Darmawan, Tadayuki Kyoutani, Ken Kaminishi

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Cab’s frame strength is considered as an important factor in excavator’s operator safety, especially during roll-over. In this study, we use a model of cab frame with different thicknesses and perform elastoplastic numerical analysis by using Finite Element Method (FEM). Deformation mode and energy absorption's of cab’s frame part are investigated on two conditions, with wrinkle and without wrinkle. The occurrence of wrinkle when deforming cab frame can reduce energy absorption, and among 4 parts with wrinkle, the energy absorption significantly decreases in part C. Residual stress that generated upon the bending process of part C is analyzed to confirm it possibility in increasing the energy absorption.

Keywords: ROPS, FEM, hydraulic excavator, cab frame

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Authors: Mehrnaz Mostafavi, Jalaledin Ghanavi

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This research investigates the production of nanoring structures through a chemical reduction approach, exploring gradual reduction processes assisted by reductant agents, leading to the formation of these specialized nanorings. The study focuses on the controlled reduction of metal atoms within these agents, crucial for shaping these nanoring structures over time. The paper commences by highlighting the wide-ranging applications of metal nanostructures across fields like Nanomedicine, Nanobiotechnology, and advanced spectroscopy methods such as Surface Enhanced Raman Spectroscopy (SERS) and Surface Enhanced Infrared Absorption Spectroscopy (SEIRA). Particularly, gold nanoparticles, especially in the nanoring configuration, have gained significant attention due to their distinctive properties, offering accessible spaces suitable for sensing and spectroscopic applications. The methodology involves utilizing human serum albumin as a reducing agent to create gold nanoparticles through a chemical reduction process. This process involves the transfer of electrons from albumin's carboxylic groups, converting them into carbonyl, while AuCl4− acquires electrons to form gold nanoparticles. Various characterization techniques like Ultraviolet–visible spectroscopy (UV-Vis), Atomic-force microscopy (AFM), and Transmission electron microscopy (TEM) were employed to examine and validate the creation and properties of the gold nanoparticles and nanorings. The findings suggest that precise and gradual reduction processes, in conjunction with optimal pH conditions, play a pivotal role in generating nanoring structures. Experiments manipulating optical properties revealed distinct responses in the visible and infrared spectrums, demonstrating the tunability of these nanorings. Detailed examinations of the morphology confirmed the formation of gold nanorings, elucidating their size, distribution, and structural characteristics. These nanorings, characterized by an empty volume enclosed by uniform walls, exhibit promising potential in the realms of Nanomedicine and Nanobiotechnology. In summary, this study presents a chemical synthesis approach using organic reducing agents to produce gold nanorings. The results underscore the significance of controlled and gradual reduction processes in crafting nanoring structures with unique optical traits, offering considerable value across diverse nanotechnological applications.

Keywords: nanoring structures, chemical reduction approach, gold nanoparticles, spectroscopy methods, nano medicine applications

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Authors: Biswajit Seal, Dushyant Kumar, Shambhu Nath, A. B. Raju

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Extension of blast furnace campaign life is highly desired for blast furnace operators mainly because of reduction of operating cost and to avoid capital expenditure cost. Tata Steel Ltd, Jamshedpur plant operates seven blast furnaces with combination of old and new technologies. The focus of Tata Steel Ltd is to push for increasing productivity with good quality product and increasing campaign life. This has been challenging for older furnaces because older furnaces are generally equipped with less automation, old design and old equipment. Good operational practices, appropriate remedial measures, and regular planned maintenance helps to achieve long campaign life of old furnaces. Good operating practices like stable and consistent productivity, control of burden distribution, remedial measures like stack gunning and shotcreting for protection of stack wall, enhanced cooling system, and intermediate stack repair helps to achieve long campaign life of old blast furnaces. This paper describes experiences with the current old equipment and design of Tata Steel’s D Blast Furnace for campaign life extension.

Keywords: blast furnace, burden distribution, campaign life, productivity

Procedia PDF Downloads 234